=29. Estimation of Lime.=—One hundred cubic centimeters of the solution
(containing one gram of the original substance) are evaporated in a
beaker to about fifty cubic centimeters; ten cubic centimeters of
dilute sulfuric acid (one to five) are added; and the evaporation is
continued on the water-bath until a considerable crop of crystals of
gypsum has formed[20]. The solution is then allowed to cool, when it
generally becomes pasty, owing to the separation of additional gypsum.
When it is cold, 150 cubic centimeters of ninety-five per cent alcohol
are slowly added, with continual stirring, and the whole is allowed
to stand for three hours, being stirred from time to time. After
three hours, it is filtered, with the aid of a filter-pump, into a
distillation flask, and the beautifully crystalline precipitate, which
does not adhere to the beaker, is washed with ninety-five per cent
alcohol. The filter, with the precipitate, is gently removed from the
funnel and inverted into a platinum crucible, so that, by squeezing the
point of the filter, the precipitate is made to fall into the crucible,
and the paper can be pressed down smoothly upon it. On gentle heating
of the crucible, the remaining alcohol burns off, and when the paper
has been completely destroyed, the heat is raised to the full power
of a bunsen for about five minutes. After cooling in a desiccator the
crucible containing the calcium sulfate, is weighed. The filtration may
also be accomplished on asbestos felt.
=30. The Ammonium Oxalate Method.=—This method has been extensively
used in this country in commercial work, and is best carried out as
described by Wyatt.[21] The total filtrates from the iron and alumina
precipitates, secured as described in paragraph =33=, are well mixed
and concentrated to a volume of about 100 cubic centimeters. There
are added about twenty cubic centimeters of a saturated solution of
ammonium oxalate, and after stirring, the mixture is allowed to cool
and remain at rest for six hours. The supernatant liquid is poured
through a filter, the residue washed three times by decantation with
hot water and brought upon the filter. The beaker and precipitate are
washed at least three times. The precipitate is dried and ignited at
low redness for ten minutes. The temperature is then raised by a blast
and the ignition continued for five minutes longer, or until the lime
is obtained as oxid. The precipitate is likely to contain magnesia. The
magnesia is estimated in the filtrates from the lime determination by
first mixing them and concentrating to 100 cubic centimeters, which,
after cooling, are made strongly alkaline with ammonia. After allowing
to stand for twelve hours the ammonium magnesium phosphate is collected
and reduced to magnesium pyrophosphate by the usual processes. If one
gram of the original material has been used the pyrophosphate obtained,
multiplied by 0.36, will give the weight of magnesia contained therein.
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